CN106756775A - A kind of alloy surface forms the preparation method of spinelle coating - Google Patents
A kind of alloy surface forms the preparation method of spinelle coating Download PDFInfo
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- CN106756775A CN106756775A CN201510831617.2A CN201510831617A CN106756775A CN 106756775 A CN106756775 A CN 106756775A CN 201510831617 A CN201510831617 A CN 201510831617A CN 106756775 A CN106756775 A CN 106756775A
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/28—Solid state diffusion of only metal elements or silicon into metallic material surfaces using solids, e.g. powders, pastes
- C23C10/34—Embedding in a powder mixture, i.e. pack cementation
- C23C10/52—Embedding in a powder mixture, i.e. pack cementation more than one element being diffused in one step
- C23C10/54—Diffusion of at least chromium
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/06—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases
- C23C10/14—Solid state diffusion of only metal elements or silicon into metallic material surfaces using gases more than one element being diffused in one step
-
- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C10/00—Solid state diffusion of only metal elements or silicon into metallic material surfaces
- C23C10/60—After-treatment
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- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
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- Organic Chemistry (AREA)
- Other Surface Treatments For Metallic Materials (AREA)
- Solid-Phase Diffusion Into Metallic Material Surfaces (AREA)
Abstract
The present invention relates to the preparation method that a kind of alloy surface forms spinelle coating; Mn, Cr alloying element are penetrated into by alloy surface using element co-penetration technology; increase the surface-element particularly concentration of Mn, then preferentially generate the manganese picotite diaphragm of densification in material surface in-situ oxidation by low oxygen partial pressure method again.The diaphragm can effectively improve resistance to high temperature oxidation, impervious carbon, the performance of anti-coking of material, so as to extend the service life or coke cleaning period of material.
Description
【Technical field】
It is that a kind of alloy surface forms spinelle coating specifically the present invention relates to coating technology field
Preparation method.
【Background technology】
The alloy of Cr, Ni constituent content high is the class material generally used under hot environment, and Cr can be carried
High antioxidant and heat resistance, Ni can improve the intensity of steel, and keep good plasticity and toughness,
There are antirust and temperature capacity under high temperature.But higher than 1000 DEG C and containing CO, CO2、H2O、
CH4、H2In hot environment Deng gas, the Cr of alloy surface containing Cr2O3Protection oxide layer is susceptible to
Volatilization, peeling, more can be that serious carburization reaction occurs in carburizing atmosphere, so as to be degrading matrix
Performance.In addition, at high temperature, chemical-process petrochina hydro carbons easily with catalytic elements Ni in alloy material,
Fe etc. interacts and deposits coking, dramatically increases heat transfer resistance, influences heat transfer.Therefore compel to be essential
To prepare to form more stable inert coatings on the surface of high-chromium-nickel alloy, so as to improve the anti-height of material
Warm oxidation, impervious carbon, anticoking capability.
In United States Patent (USP) US7156979, NOVA companies use hydrogen and vapor mixed atmosphere, in
800-1100 DEG C is prepared one layer of Mn in stainless steel surfacesxCr3-xO4(0.5≤x≤1.5) spinel structure is protected
Film.In Chinese patent CN102719783A, CN101565807A, CN101565808A, use
In-situ oxidation method, reaction process in tube skin under high temperature in preparing Mn in one or two stepsxCr3-xO4
(0.5≤x≤1.5) spinelle coating.A certain proportion of inorganic matter is sprayed on boiler tube inwall by US6423415
Sintering forms ceramic coating.CN201010286801.0, CN201010286788.9 etc. are in furnace tube material
Add the elements such as rare earth element or Al, Si, B to be prepared using low oxygen partial pressure method and suppress coking coating.
Certain protective effect can be played to matrix using the standby spinelle protective layer of above-mentioned patent system, but
Have the following disadvantages:Alloy material matrix Mn constituent contents are about 1% or so, and surface is formed preferably
Mn contents are up to 24% or 34% (not considering O elements) in spinel layer, simple by matrix
Mn elements to the spinelle coating prepared by external diffusion than relatively thin, and not preferably stoicheiometry
MnCr2O4;Ceramic coating differs larger with furnace tube material performance, and coating life is shorter;The easy scaling loss of rare earth,
Element influences boiler tube mechanical performance and the welding performances such as intrinsic silicon Al, Si higher.
【The content of the invention】
It is an object of the invention to overcome the deficiencies in the prior art, there is provided a kind of alloy surface forms spinelle
The preparation method of coating;It is dense that the application regulates and controls alloy material surface Cr, Mn element by element co-penetration technology
Degree distribution, then preferentially formed in alloy material surface original position under the conditions of low oxygen partial pressure fine and close, stabilization
MnCr2O4Spinelle diaphragm, is effectively improved the resistance to high temperature oxidation of alloy material, impervious carbon, anti-
Coking behavior.
The purpose of the present invention is achieved through the following technical solutions:
A kind of alloy surface forms the preparation method of spinelle coating, and it is concretely comprised the following steps:
(1) alloy material surface is done into degreasing and rust removal pretreatment:
By percentage to the quality, Cr is that 0.1~50%, Mn is 0.1~5% to described alloy material composition,
Ni is that 20~50%, Si is 0.2~3%, and trace element is 0.01~5%, balance of Fe;
Trace element includes one or more in Nb, Ti, W, Al, C, rare earth element, typically
Material trademark is HP40, HK40,35Cr45Ni, Incoloy 800,25Cr20Ni, 326L.
(2) Mn, Cr permeation are carried out to alloy material using powder pack cementation or the method for gas phase permeation
Treatment;
The composition of the penetration enhancer of powder embedding cementation process by percentage to the quality, chromium powder or ferrochrome powder be 10~
60%, manganese powder or ferromanganese powder are 2~40%, and ammonium chloride is 1~5%, and sodium fluoride is 0.2~1%, oxidation
Cerium is 0.1~0.5%, balance of Al2O3Powder;
The powder of penetration enhancer is 50~500 mesh;
The heating-up temperature of powder embedding cementation process is 800~1100 DEG C, preferably 900~1100 DEG C;
The heat time of powder embedding cementation process is 1~10h, preferably 5~8h;
By percentage to the quality, chromium powder or ferrochrome powder are 30~60%, manganese in solid phase source in gas phase co-penetration technology
Powder or ferromanganese powder are 10~30%, and cerium oxide is 0.1~0.5%, and sodium fluoride is 0.2~1%, balance of
Al2O3;
Gaseous sources used are:H2With HCl gaseous mixtures, wherein in gaseous mixture volume fraction shared by HCl be 10~
80%, preferably 40~60%;
The heating-up temperature of gas phase permeation is 800~1100 DEG C, preferably 950~1050 DEG C;
The heating treatment time of gas phase permeation is 1~8h, preferably 3~6h;
The co-penetration layer prepared mainly is made up of elements such as Cr, Mn, Fe, Ni, Si, co-penetration layer Mn's
Molar fraction is 30~60%, balance of matrix other elements for the molar fraction of 4~20%, Cr;
Cocementation layer depth is 5~20 μm;
(3) alloy material surface after permeation is cleared up, it is 30~50% to use mass percent
NaOH the or KOH aqueous solution carries out alkali cleaning;
(4) water vapour is introduced into vector gas using Bubbling method, then mixed gas is passed through is equipped with
In the heat-treatment furnace of alloy material, the temperature of bubbling electrolyte solution is by thermostatical water bath control;
Vector gas are selected from one or more in hydrogen, nitrogen, argon gas;
The molar fraction of vapor is 0.1~5% in mixed gas;
(5) furnace temperature is risen into 700~1200 DEG C carries out high-temperature oxydation, and the temperature of high-temperature oxydation is preferably
950~1100 DEG C, 5~15h is incubated, the soaking time of high-temperature oxydation is preferably 6~10h;
(6) furnace cooling or room temperature or less than 150 DEG C are cooled to the speed of 5~30 DEG C/min, is closed
Hold one's breath body, obtain 5~20 μm of spinelle coatings.
The outer layer of spinelle coating is spinel layer, and composition is MnCr2O4;The internal layer of spinelle coating is
The composite oxide layer of chromium oxide, silica etc..
Compared with prior art, the positive effect of the present invention is:
(1) formed in the technology of spinel-like diaphragm, Mn elements are from alloy substrate, and base
Mn contents in body are very low, and only 1~2% or so.Manganese picotite is outside by Mn elements in matrix
Diffusing to the chromium oxide that Cr, the O in outer surface and outside generate react formation, therefore formed
Spinelle thickness of thin, usual 1~3 micron.And the Mn in the present invention is mainly derived from diffusion medium, through altogether
Ooze rear substantial amounts of Mn elements and be present in alloy material top layer, for the formation of spinelle provides substantial amounts of manganese
Source, so as to improve the formation speed of spinelle and the thickness of coating.
(2) Cr, Mn permeation can prevent from oozing the local manganese element too high levels that manganese causes merely, hypoxemia point
Substantial amounts of loose manganese oxide quickly preferentially generates and peels off or can not form preferable stoicheiometry during pressure oxidation
MnCr2O4.The present invention can control surface well by allocating the method for Mn, Cr penetration enhancer ratio permeation
The concentration distribution of Mn elements in infiltration layer.
(3) NaOH or KOH alkali cleanings are used after alloy surface permeation, when can thoroughly remove element permeation
The surface such as produced chromium oxide, aluminum oxide firm attachment thing so that follow-up low oxygen partial pressure forms spinelle
Dense structure is smooth, high with substrate combinating strength.
(4) because Mn, Cr co-penetration layer have certain thickness, it is brilliant that it can quickly provide generation chromium manganese point
A large amount of Mn elements required for stone coating, moreover, may also function as regenerating the effect of selfreparing, repair
The spinelle coating being deteriorated during use.
【Brief description of the drawings】
The cross-sectional morphology figure of infiltration layer after Figure 1A HP40 permeations;
The EDS distribution diagram of element of infiltration layer after Figure 1B HP40 permeations;
Fig. 2 face coat XRD constituent analysis figures;
Fig. 3 face coat patterns SEM schemes;
Fig. 4 face coat elementary analyses EDS schemes;
Fig. 5 coating cross sections patterns SEM schemes.
【Specific embodiment】
A kind of alloy surface of the invention presented below forms the specific embodiment party of the preparation method of spinelle coating
Formula.
Embodiment 1
Example is prepared for fine and close, uniform and with certain thickness MnCr in HP40 alloy surfaces2O4
Spinelle coating.
After by HP40 alloy material surface degreasing and rust removals, it is put into together with pack cementation penetration enhancer in oozing tank, penetration enhancer
Quality percentage is calculated as:Chromium powder 25%, ferromanganese powder (iron-holder 40%) 30%, ammonium chloride 1.5%, fluorination
Sodium 0.4%, cerium oxide 0.2%, balance of Al2O3Powder.Ooze tank to be sealed with fire clay, then will ooze tank and put
Enter and carry out permeation heat treatment in Muffle furnace.Muffle furnace heat treatment temperature is 1050 DEG C, soaking time 5h, drop
Warm speed is 10 DEG C/min.Treat that in-furnace temperature is down to 100 DEG C, tank is oozed in taking-up, by HP40 alloy material tables
Face is cleared up with clear water after the NaOH aqueous solution soakings of 30% concentration, then is placed in Tubular thermal treatment furnace.Hydrogen
Used as carrier gas, gas flow rate is 100ml/min, and first Bubbling method flows through deionized water, and coolant-temperature gage is 20
DEG C, then it is passed through in Tubular thermal treatment furnace again.1050 DEG C are heated to the heating rate of 15 DEG C/min, are protected
Warm 8h, insulation cools to 100 DEG C with the furnace after terminating, close carrier gas.Through permeation and hypoxemia oxidation processes
Afterwards, alloy material surface forms fine and close, the uniform and MnCr with higher caliper2O4Spinelle coating.
The HP40 material co-penetration layer cross-sectional morphologies and EDS distribution diagram of element obtained by permeation treatment are such as
Shown in Fig. 1.Surface co-penetration layer has formd certain thickness rich Cr, Mn, poor Fe, Ni layer.Surface
The XRD analysis of coating are as shown in Figure 2.Surface alloy surface forms the whole MnCr of comparing2O4Spinelle
Coating.Fig. 3 is the surface topography of coating, and coating surface is uniform, fine and close.Fig. 4 is coating surface EDS
Elementary analysis, coating is made up of Mn, Cr, O element, while having confirmed surface for MnCr2O4Spinelle.
The coating composition can effectively suppress oxidation, carburizing and coking under material at high temperature carburizing environment, extend material
The service life or coke cleaning period of material, can reduce ethylene cracking tube coking amount using the method for the present invention
More than 70%.
The above is only the preferred embodiment of the present invention, it is noted that general for the art
Logical technical staff, without departing from the inventive concept of the premise, can also make some improvements and modifications,
These improvements and modifications also should be regarded as in protection scope of the present invention.
Claims (10)
1. a kind of alloy surface forms the preparation method of spinelle coating, it is characterised in that its specific steps
For:
(1) alloy material surface is done into degreasing and rust removal pretreatment:
(2) Mn, Cr permeation are carried out to alloy material using powder pack cementation or the method for gas phase permeation
Treatment;
The composition of the penetration enhancer of powder embedding cementation process by percentage to the quality, chromium powder or ferrochrome powder be 10~
60%, manganese powder or ferromanganese powder are 2~40%, and ammonium chloride is 1~5%, and sodium fluoride is 0.2~1%, oxidation
Cerium is 0.1~0.5%, balance of Al2O3Powder;
By percentage to the quality, chromium powder or ferrochrome powder are 30~60%, manganese in solid phase source in gas phase co-penetration technology
Powder or ferromanganese powder are 10~30%, and cerium oxide is 0.1~0.5%, and sodium fluoride is 0.2~1%, balance of
Al2O3;
(3) alloy material surface after permeation is cleared up, it is 30~50% to use mass percent
NaOH the or KOH aqueous solution carries out alkali cleaning;
(4) water vapour is introduced into vector gas using Bubbling method, then mixed gas is passed through is equipped with
In the heat-treatment furnace of alloy material, the temperature of bubbling electrolyte solution is by thermostatical water bath control;
(5) furnace temperature is risen into 700~1200 DEG C carries out high-temperature oxydation, and the temperature of high-temperature oxydation is preferably
950~1100 DEG C, 5~15h is incubated, the soaking time of high-temperature oxydation is preferably 6~10h;
(6) furnace cooling or room temperature or less than 150 DEG C are cooled to the speed of 5~30 DEG C/min, is closed
Hold one's breath body, obtain 5~20 μm of spinelle coatings.
2. a kind of alloy surface as claimed in claim 1 forms the preparation method of spinelle coating, and it is special
Levy and be, in described step (1), described alloy material composition by percentage to the quality, Cr
Be 0.1~50%, Mn for 0.1~5%, Ni is that 20~50%, Si is 0.2~3%, trace element for 0.01~
5%, balance of Fe;
Trace element includes one or more in Nb, Ti, W, Al, C, rare earth element.
3. a kind of alloy surface as claimed in claim 1 forms the preparation method of spinelle coating, and it is special
Levy and be, in described step (2), the heating-up temperature of powder embedding cementation process is 800~1100 DEG C,
Preferably 900~1100 DEG C.
4. a kind of alloy surface as claimed in claim 1 forms the preparation method of spinelle coating, and it is special
Levy and be, in described step (2), the heat time of powder embedding cementation process is 1~10h, excellent
Elect 5~8h as.
5. a kind of alloy surface as claimed in claim 1 forms the preparation method of spinelle coating, and it is special
Levy and be, in described step (2), gaseous sources used are:H2With HCl gaseous mixtures, wherein mixing
Volume fraction shared by HCl is 10~80%, preferably 40~60% in gas.
6. a kind of alloy surface as claimed in claim 1 forms the preparation method of spinelle coating, and it is special
Levy and be, in described step (2), the heating-up temperature of gas phase permeation is 800~1100 DEG C, preferably
It is 950~1050 DEG C.
7. a kind of alloy surface as claimed in claim 1 forms the preparation method of spinelle coating, and it is special
Levy and be, in described step (2), the heating treatment time of gas phase permeation is 1~8h, preferably
3~6h.
8. a kind of alloy surface as claimed in claim 1 forms the preparation method of spinelle coating, and it is special
Levy and be, in described step (2), the co-penetration layer prepared it is main by Cr, Mn, Fe, Ni,
The elements such as Si are constituted, and the molar fraction of co-penetration layer Mn is 30~60% for the molar fraction of 4~20%, Cr,
Balance of matrix other elements;
Cocementation layer depth is 5~20 μm.
9. a kind of alloy surface as claimed in claim 1 forms the preparation method of spinelle coating, and it is special
Levy and be, in described step (4), vector gas be selected from hydrogen, nitrogen, argon gas in one kind or
It is several;
The molar fraction of vapor is 0.1~5% in mixed gas.
10. a kind of alloy surface as claimed in claim 1 forms the preparation method of spinelle coating, and it is special
Levy and be, in described step (6), the outer layer of spinelle coating is spinel layer, and composition is MnCr2O4;
The internal layer of spinelle coating is the composite oxide layer of chromium oxide, silica etc..
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107164722A (en) * | 2017-06-23 | 2017-09-15 | 江苏双勤民生冶化设备制造有限公司 | A kind of alloy surface coating and preparation method thereof |
CN109226751A (en) * | 2018-11-28 | 2019-01-18 | 湖南科技大学 | A kind of polynary Fe-Si alloy coat of vacuum non-pressure sintering and preparation method thereof |
CN109267114A (en) * | 2018-10-22 | 2019-01-25 | 中国科学院金属研究所 | A kind of preparation method of cobalt-manganese spinel coating |
CN112853260A (en) * | 2021-01-09 | 2021-05-28 | 华东理工大学 | Preparation method of powder embedding infiltration coating |
CN114427071A (en) * | 2020-10-15 | 2022-05-03 | 中国石油化工股份有限公司 | Alloy surface treatment method, alloy and application |
CN115287529A (en) * | 2022-08-16 | 2022-11-04 | 河北科技大学 | Nickel-iron-based alloy coating and preparation method and application thereof |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN107164722A (en) * | 2017-06-23 | 2017-09-15 | 江苏双勤民生冶化设备制造有限公司 | A kind of alloy surface coating and preparation method thereof |
CN109267114A (en) * | 2018-10-22 | 2019-01-25 | 中国科学院金属研究所 | A kind of preparation method of cobalt-manganese spinel coating |
CN109226751A (en) * | 2018-11-28 | 2019-01-18 | 湖南科技大学 | A kind of polynary Fe-Si alloy coat of vacuum non-pressure sintering and preparation method thereof |
CN114427071A (en) * | 2020-10-15 | 2022-05-03 | 中国石油化工股份有限公司 | Alloy surface treatment method, alloy and application |
CN112853260A (en) * | 2021-01-09 | 2021-05-28 | 华东理工大学 | Preparation method of powder embedding infiltration coating |
CN115287529A (en) * | 2022-08-16 | 2022-11-04 | 河北科技大学 | Nickel-iron-based alloy coating and preparation method and application thereof |
CN115287529B (en) * | 2022-08-16 | 2023-08-18 | 河北科技大学 | Nickel-iron-based alloy coating and preparation method and application thereof |
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